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Process for the preparation of concentrated solutions of stabilized hypobromites

a concentrated solution and stabilized technology, applied in the field of concentrated solution preparation of stabilized hypobromites, can solve the problems of slow precipitation, insufficient stable for practical and commercial application, and the disadvantage of yielding equivalent amounts of naobr and nacl of hypochlorite, and achieve the effect of higher stability

Inactive Publication Date: 2011-05-10
BROMINE COMPOUNDS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0024]The aqueous solution obtained is free from alkali chloride. It contains, depending on the concentration of the sulfamic acid or sulfamate solution, an amount of active halogen, expressed as available chlorine, from 7 to 11.5 wt %, based on the weight of the whole solution and determined by iodometric titration. The solution prepared by the process defined hereinbefore, has a higher stability than the solution of the prior art, as will be specified later on.

Problems solved by technology

However, the precipitation is slow.
This mode of operation enables the preparation of MOBr solution (M=Na, K), but these are not stable enough for practical and commercial application.
The reaction with hypochlorite has the disadvantage of yielding equivalent amounts of NaOBr and NaCl.
The strong oxidizing potential of the hypobromous acid and hypobromites made them very difficult to stabilize.
However, some strong oxidants, among them chlorine and bromine, can attack the NH2 function liberating nitrogen.
However, since hypochlorite solutions generally contain chlorides in an equivalent amount with hypochlorites, the resulting mixtures contain large amounts of sodium chloride.
It does not teach the preparation of hypobromite solutions.
Bromine chloride is difficult to handle and tends to dissociate to bromine and chlorine.
It is not a commercial product and must be manufactured by using special skills and expensive installations for keeping it in liquid phase under pressure.

Method used

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  • Process for the preparation of concentrated solutions of stabilized hypobromites
  • Process for the preparation of concentrated solutions of stabilized hypobromites

Examples

Experimental program
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example 1

[0035]A concentrated hypobromite solution was prepared by contacting, under vigorous stirring, a mixture of 532.5 g of a concentrated aqueous NaOH solution (49.2 wt %) and 494 g water with 480 g bromine, while adding gradually so that the temperature is maintained at 0±5° C. The NaOH / bromine molar ratio was 2.2:1. A clear, dark yellow solution of unstabilized sodium hypobromite was obtained, which contained 23.2 wt % NaOBr and 20.5 wt % NaBr. In spite of the very high concentration and low temperature, no precipitation occurred due to the very high solubility of NaBr. To the above hypobromite solution, an aqueous solution of sodium sulfamate was added gradually, in order to keep the temperature between −5 to 10° C., preferably 0-5° C.

[0036]The above said aqueous solution of sodium sulfamate was prepared by gradually adding at room temperature 401.7 g of an aqueous 49.2 wt % NaOH solution to 836.5 g of an aqueous slurry composed of 436.5 g sulfamic acid and 400 g water, was added to ...

example 2

[0038]In a reactor provided with cooling jacket and mixing device, introduced was 500 g stabilized bromine solution prepared as described in Example 1. To this solution, cooled at 0-5° C., was added 377 g of a sodium hypochlorite commercial solution containing 11% sodium hypochlorite (expressed as available chlorine) that reacted with the NaBr present, forming NaOBr. The solution in the reactor (877 g) then contained ca 14.6% NaOBr, practically no NaBr, 4.6% NaCl and 10.9% sulfamate. The solution can be utilized as such but it is less stable on storage because the ratio between sulfamate and hypobromite is less than required. This solution contained 8.8% available halogen (as Cl2).

example 3

[0039]A more stable, but less concentrated, stabilized bromine solution was prepared by adding, at 0-10° C., to the mixture prepared as in Example 2, 222 g sodium sulfamate, prepared as in Example 1. The 1109 g solution thus obtained contained ca 11.5 wt % sodium hypobromite. In terms of available chlorine it contained ca 7% available chlorine. The molar ratio of sodium sulfamate to NaOBr in this solution was 1.5:1.

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Abstract

The invention provides stabilized concentrated aqueous solutions of alkali hypobromites, as well as a process for the preparation of said stabilized concentrated solutions at low temperatures, comprising reacting a concentrated alkali hydroxide aqueous solution with bromine, adding to the non-stabilized reaction product an aqueous solution of a sulfamic compound to stabilize the hypobromite, and oxidizing bromide to produce additional hypobromite.

Description

CLAIM OF PRIORITY[0001]This application claims priority as a continuation in part application of U.S. patent application Ser. No. 12 / 353,401 filed on Jan. 14, 2009; which is a continuation-in-part application of U.S. patent application Ser. No. 10 / 513,512 having a 371(c) date of Jun. 20, 2005 (submitted to the USPTO on Nov. 4, 2004); which is a 371 of PCT / IL2003 / 000363, filed on May 5, 2003; which claims priority to Israeli patent application serial number 149499, filed on May 6, 2002.FIELD OF THE INVENTION[0002]This invention relates to a method for the preparation of concentrated solutions of stabilized hypobromites. This invention also relates to stabilized solutions of hypobromites obtained by the process of this invention.BACKGROUND OF THE INVENTION[0003]Hypobromous acid is one of the most potent sanitizers among the oxidizing halogenated compounds. Since it is a weaker acid than hypochlorous acid (pK=8.8 at 25° C.), it is predominant at pH higher than 9.[0004]Alkaline hypobrom...

Claims

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Application Information

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Patent Type & Authority Patents(United States)
IPC IPC(8): C01B11/20C02F1/76
CPCC01B11/20C02F1/766C01D3/10C02F1/722
Inventor FISHLER, THEODOR MORELFELDMAN, DAVID
Owner BROMINE COMPOUNDS
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